CN110272270A - A kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics and preparation method thereof - Google Patents

A kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics and preparation method thereof Download PDF

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CN110272270A
CN110272270A CN201910582277.2A CN201910582277A CN110272270A CN 110272270 A CN110272270 A CN 110272270A CN 201910582277 A CN201910582277 A CN 201910582277A CN 110272270 A CN110272270 A CN 110272270A
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temperature
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preparation
dielectric loss
piezoelectric ceramics
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CN110272270B (en
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杨华斌
刘笑
黄蔚然
孙媛媛
陈巧红
江民红
张秀云
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Guilin University of Electronic Technology
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Abstract

The invention discloses a kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics and preparation method thereof, formula composition general formula is (Bi1‑w M w )(Fe1‑ t Me''' t )O3‑xBaTiO3+yBi(Me'0.5Me''0.5)O3+zBi(Zn0.5Ti0.5)O3+uNdCoO3 +mP+nMnCO3, whereinx、y、z、 u、m、n、t、wExpression molar fraction, 0 <x≤ 0.4,0≤y≤ 0.1,0 <z< 0.05,0≤u≤ 0.1,0 <m≤ 0.1,0 <n≤ 0.1,0≤w≤0.1、0≤t≤0.1.M, Me''' are trivalent metallic element in formula, and Me'', M' are respectively divalent, pentagonal metal element, and P is sintering aid.The piezoelectric ceramics has low-dielectric loss and high-temperature stability, can be applied to high-temperature field.

Description

A kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high temperature Leadless piezoelectric ceramics and preparation method thereof
Technical field
The present invention relates to a kind of high-temp leadless piezoelectric ceramics and preparation method thereof, it is specifically a kind of have low-dielectric loss and The bismuth ferrite of high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics and preparation method thereof.
Background technique
High-temperature piezoelectric ceramics are widely used in the piezoelectric vibration sensors in the fields such as space flight and aviation, nuclear energy, oil exploration. BiFeO3-BaTiO3System piezoelectric ceramics is because its is unleaded, sintering temperature is low, Curie temperature is high, depolarization temperature is high and good Piezoelectric property etc. receives great attention.But the system answer it can not actually always since dielectric loss is higher always With, therefore the dielectric loss of the system how is reduced, it is that the system is able to the key technology applied in high-temperature field.
BF-BT(BiFeO3-BaTiO3) dielectric loss of system mainly causes by the factor of the following aspects:
(1) due to pure BiFeO3Sintering temperature be 800 DEG C or so, and BaTiO3Sintering temperature be 1450 DEG C or so, two Person's difference reaches 650 DEG C, therefore, in order to improve BiFeO3-BaTiO3The consistency and performance of ceramic systems, it has to will be sintered Temperature is increased to 1000 DEG C or so, and Bi element highly volatile at these elevated temperatures, so that sintered products deviate design Stoichiometric ratio, and lead to the generation of Lacking oxygen；
(2)Fe3+Ion appraises at the current rate, in temperature-fall period, Fe3+Ion has part that can be transformed into Fe2+Ion, for maintenance Conjunction valence balance, also results in the generation of Lacking oxygen.The generation of a large amount of Lacking oxygens finally makes the leakage electrical conduction current of sample high, causes Polarization is difficult.
Document [Serhiy O, J Am Ceram Soc, 2009,92 (12): 2957-2961], which has been reported to have, is in inner temperature The BiFeO of degree and good piezoelectric property3–BaTiO3Based leadless piezoelectric ceramics, but need to be sintered in pure oxygen atmosphere, be not suitable for Industrialization production, and its piezoelectric constant is lower, only 116pC/N；Document [Ichiro Fujii, J Appl Phys, 2011, 50:09ND07] report a kind of BaTiO that Mn is adulterated3-Bi(Mg1/2Ti1/2)O3-BiFeO3Leadless piezoelectric ceramics, but piezoelectricity The best local Curie temperature of performance only has 470 DEG C, best piezoelectric constant d33Only 94pC/N does not report depolarization temperature With temperature stability；Document [Dae Su Kim, Appl.Phys.Lett.109,202902 (2016)] is reported using in air Middle quenching technical, piezoelectric property have been increased to 140pC/N from 70pC/N, can significantly improve piezoelectric property, but do not report Dielectric loss and temperature stability；Document [Yongquan Guo, J Mater Sci:Mater Electron, 2017,28: 5531-5547] NdCoO is reported3The BFBT piezoelectric ceramics of doping vario-property, and obtain d33=110pC/N or so, Curie temperature 605 DEG C, the piezoelectric ceramics that depolarization temperature is 525 DEG C, but at 525 DEG C of depolarization point, piezoelectric property only has 80pC/N, And dielectric loss is higher, is up to 7% or more in the best loss at branch of performance.
From the point of view of the research of forefathers, the dielectric loss of BF-BT system fails to obtain effective solution, therefore the system always It is the dielectric loss for how controlling the system in the key that high-temperature piezoelectric field is able to apply, this research bottleneck is broken through, to height The progress of temperature and pressure electric material will be of great significance.
Summary of the invention
For reducing the research of dielectric loss consumption, few people reduce sintering temperature using the method for addition sintering aid, subtract Few Bi element evaporation and then the purpose for realizing inhibition Lacking oxygen generation.The purpose of the present invention is be directed to BiFeO3-BaTiO3System Deficiency in the presence of preparation process, and a kind of bismuth ferrite-barium titanate with low-dielectric loss and high-temperature stability is provided Base high-temperature leadless piezoelectric ceramics and preparation method thereof.Dielectric loss is effectively reduced to 1.0% hereinafter, and keeping high by the present invention Piezoelectric property and high-temperature stability, so that BiFeO3-BaTiO3System piezoelectric ceramics can really be applied in high-temperature field.
Realizing the technical solution of the object of the invention is:
A kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics, matches Fang Zucheng general formula are as follows:
(a)、(Bi1-wMw)(Fe1-tMe”'t)O3-xBaTiO3+yBi(Me'0.5Me”0.5)O3+zBi(Zn0.5Ti0.5)O3+ uNdCoO3+mP+nMnCO3, or
(b)、(Bi1-wMw)(Fe1-tMe”'t)O3-xBaTiO3+yBi(Me”2/3M'1/3)O3+zBi(Zn0.5Ti0.5)O3+ uNdCoO3+mP+nMnCO3；
Wherein x, y, z, u, m, n, w, t expression molar fraction, 0 < x≤0.4,0≤y≤0.1,0 < z < 0.05,0≤u≤ 0.1,0 < m≤0.1,0 < n≤0.1,0≤w≤0.1,0≤t≤0.1, M is one or more of La, Er, Sm, Gd in formula, Me " ' is one or more of trivalent metallic element Sc, In, Co and Ga, and Me' is tetravalent metal elements Zr, Sn, Ti, Ge and Hf One of, Me " is one of divalent metal element Ni, Mg, Zn, Sr, Pd, one of M' Nb, Ta, Sb, V, wherein P For B2O3、Li2CO3、V2O5、CuO、CeO2、LiBiO3、Ba(Cu1/3Nb2/3)O3、Ba(W0.5Cu0.5)O3One of or a variety of burnings The combination of auxiliary agent is tied, and must wherein contain Li2CO3。
Above-mentioned bismuth ferrite-barium phthalate base high-temp leadless piezoelectric ceramics preparation with low-dielectric loss and high-temperature stability Method includes the following steps:
(1) ingredient is carried out according to the component ratio of formula (a) or formula (b)；
(2) it is medium by mixed-powder ball milling 24 hours of step (1) using dehydrated alcohol, in drying in 100 DEG C/6 hours, puts Enter high alumina crucible and compacting, cover, place into Muffle furnace with the heating rate of 250 DEG C/h to 800 DEG C, keeps the temperature 4 hours and synthesize, And cooling down is taken out afterwards to 200 DEG C or less；
(3) powder of step (2) synthesis is carried out taking out drying using dehydrated alcohol as medium secondary ball milling 24 hours；
(4) by after drying powder be added mass percent concentration be 5%PVA solution be granulated, in punching block in Compression moulding under 100MPa, mold interior diameter are 1cm；
(5) molding plain piece is to slowly warm up to 600 DEG C in tube furnace with the heating rate of 30 DEG C/h, keeps the temperature dumping for 24 hours, Then with the heating rate of 20 DEG C/min to 980-1000 DEG C, 120min is kept the temperature, then power-off cools to room temperature with the furnace；
(6) sintered sample is processed into two sides is smooth, thin slice of thickness 1mm, drapes over one's shoulders silver electrode, 600 DEG C/30min is burnt It is spare after silver；
(7) piezoelectric ceramic piece of preparation is polarized in silicone oil, polarized electric field 6000V/mm, 150 DEG C of temperature, the time 30 divides Clock keeps electric field to be cooled to room temperature.
The positive effect of the present invention is:
The present invention has successfully prepared the high-temp leadless piezoelectric ceramics with low-dielectric loss and high-temperature stability, obtains Dielectric loss is down to that 1.0% or less, piezoelectric constant reaches 100pC/N or more, Curie temperature is more than 630 DEG C, depolarization temperature The BF-BT high-temp leadless piezoelectric ceramics that reaches 610 DEG C or more, can be applied in high-temperature field.This preparation method simple process, no High-temperature and high-pressure conditions synthetic powder and pure oxygen atmosphere is needed to be sintered, and function admirable, this is for BiFeO3-BaTiO3System pressure For electroceramics, there is important breakthrough and technical innovation, can be applied completely in space flight and aviation, nuclear energy, oil exploration etc. Key areas.
Detailed description of the invention
Fig. 1 is the depolarization curve graph of the piezoelectric ceramics prepared in embodiment 2.
Specific embodiment
By example given below, the contents of the present invention can be further apparent from, but they are not to this The restriction of invention.
Embodiment 1:
It is formulated (b) ingredient:
(Bi0.995La0.005)(Fe0.97Ga0.03)O3-0.25BaTiO3+0.01Bi(Mg2/3Nb1/3)O3+0.03Bi (Zn0.5Ti0.5)O3+0.01NdCoO3+0.01Ba(W0.5Cu0.5)O3+0.01Li2CO3+0.01MnCO3, preparation method includes as follows Step:
(1) to analyze pure Bi2O3、Fe2O3、La2O3、Ga2O3、BaCO3、TiO2、MgO、Nb2O3、ZnO、Nd2O3、Co2O3、 WO3、CuO、Li2CO3、MnCO3For raw material, ingredient is carried out according to formula rate；
(2) using dehydrated alcohol as medium by the mixed-powder ball milling 24 of step (1) it is small and when, 100 DEG C/6 hours dry； Powder is put into high alumina crucible and compacting again, is covered, is placed into Muffle furnace with the heating rate of 250 DEG C/h to 800 DEG C, is kept the temperature It synthesizes within 4 hours, and cooling down is taken out afterwards to 200 DEG C or less；
(3) powder of step (2) synthesis is carried out taking out drying using dehydrated alcohol as medium secondary ball milling 24 hours；
(4) by after drying powder be added mass percent concentration be 5%PVA solution be granulated, in punching block in Compression moulding under 100MPa, mold interior diameter are 1cm；
(5) molding plain piece is to slowly warm up to 600 DEG C with the heating rate of 30 DEG C/h, dumping for 24 hours is kept the temperature, then with 20 DEG C/heating rate of min to 980 DEG C, keep the temperature 120min, then power-off cools to room temperature with the furnace；
(6) sintered sample is processed into two sides is smooth, thin slice of thickness 1mm, drapes over one's shoulders silver electrode, 600 DEG C/30min is burnt It is spare after silver；
(7) piezoelectric ceramic piece of preparation is polarized in silicone oil, polarized electric field 6000V/mm, 150 DEG C of temperature, the time 30 divides Clock keeps electric field to be cooled to room temperature.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
97 143.2 0.314 630 610 0.973
Embodiment 2:
It is formulated (a) ingredient:
Bi(Fe0.97Ga0.03)O3-0.25BaTiO3+0.01Bi(Ti0.5Mg0.5)O3+0.03Bi(Zn0.5Ti0.5)O3+ 0.01NdCoO3+0.01Li2CO3+0.005CuO+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、Ga2O3、BaCO3、TiO2、MgO、ZnO、Nd2O3、Co2O3、CuO、Li2CO3、 MnCO3For raw material, ingredient is carried out according to formula rate；
For other steps with embodiment 1, sintering temperature is 970 DEG C.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
102 129.6 0.328 626 605 0.945
It will be noted from fig. 1 that potsherd obtains d after 150 DEG C, 6000V/mm electric field polarization33=102pC/N's Piezoelectric property has a step in 440 DEG C of depolarizations, and with the increase of depolarization temperature, at 610 DEG C, there are also d33= The piezoelectric property of 80pC/N.
Embodiment 3:
It is formulated (b) ingredient:
Bi(Fe0.98Sc0.02)O3-0.3BaTiO3+0.025Bi(Zn2/3V1/3)O3+0.025Bi(Zn0.5Ti0.5)O3+ 0.01NdCoO3+0.01Li2CO3+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、Sc2O3、BaCO3、TiO2、ZnO、V2O5、Nd2O3、Co2O3、Li2CO3、MnCO3For Raw material carries out ingredient according to formula rate；
Other steps are the same as embodiment 1.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
97 116.6 0.301 618 605 0.934
Embodiment 4:
It is formulated (b) ingredient: Bi (Fe0.99Co0.01)O3-0.25BaTiO3+0.01Bi(Zn2/3Nb1/3)O3+0.025Bi (Zn0.5Ti0.5)O3+0.01NdCoO3+0.01Li2CO3+0.008CuO+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、BaCO3、TiO2、ZnO、Nb2O5、Nd2O3、Co2O3、CuO、Li2CO3、MnCO3For Raw material carries out ingredient according to formula rate；
Other steps are the same as embodiment 1.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
92 96.6 0.288 623 602 0.963
Embodiment 5:
It is formulated (a) ingredient:
Bi(Fe0.97Ga0.03)O3-0.25BaTiO3+0.01Bi(Ti0.5Mg0.5)O3+0.03Bi(Zn0.5Ti0.5)O3+ 0.01Li2CO3+0.01Cu O+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、Ga2O3、BaCO3、TiO2、MgO、ZnO、Li2CO3、CuO、MnCO3For raw material, press Ingredient is carried out according to formula rate；
Other steps are the same as embodiment 1.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
93 117.6 0.301 590 575 0.998
Embodiment 6:
It is formulated (a) ingredient:
Bi(Fe0.97In0.03)O3-0.30BaTiO3+0.01Bi(Ti0.5Mg0.5)O3+0.03Bi(Zn0.5Ti0.5)O3+ 0.01NdCoO3+0.01Li2CO3+0.01CuO+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、In2O3、BaCO3、TiO2、MgO、ZnO、Nd2O3、Co2O3、CuO、Li2CO3、 MnCO3For raw material, ingredient is carried out according to formula rate；
Other steps are the same as embodiment 1.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
87 104.4 0.298 595 575 0.913
Embodiment 7:
It is formulated (a) ingredient:
Bi(Fe0.98Sc0.02)O3-0.30BaTiO3+0.01Bi(Ti0.5Mg0.5)O3+0.03Bi(Zn0.5Ti0.5)O3+ 0.01NdCoO3+0.01Li2CO3+0.005CuO+0.01MnCO3,
Preparation method comprises the following steps:
(1) to analyze pure Bi2O3、Fe2O3、Sc2O3、BaCO3、TiO2、MgO、ZnO、Nd2O3、Co2O3、CuO、Li2CO3、 MnCO3For raw material, ingredient is carried out according to formula rate；
Other steps are the same as embodiment 1.
Performance measurements are as follows:
d33(pC/N) Qm kp(%) Tc(℃) Td(℃) Tan δ (%)
81 109.6 0.306 590 570 0.965
The bound of ingredient cited by the present invention, the bound of section value and technological parameter, section value can Realize the present invention, implementation numerous to list herein.

Claims (4)

1. a kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics, feature It is, forms general formula are as follows: (Bi1-wMw)(Fe1-tMe”'t)O3-xBaTiO3+yBi(Me'0.5Me”0.5)O3+zBi(Zn0.5Ti0.5) O3+uNdCoO3+mP+nMnCO3, wherein x, y, z, u, t, m, n, w indicate molar fraction, 0 < x≤0.4,0≤y≤0.1,0 < z < 0.05,0≤u≤0.1,0 < m≤0.1,0 < n≤0.1,0≤w≤0.1,0≤t≤0.1, M is one in La, Er, Sm, Gd in formula Kind or it is several, Me " ' is one or more of trivalent metallic element Sc, In, Co and Ga, Me' be tetravalent metal elements Zr, Sn, One of Ti, Ge and Hf, Me " are one of divalent metal element Ni, Mg, Zn, Sr, Pd, and wherein P is B2O3、Li2CO3、 V2O5、CuO、CeO2、LiBiO3、Ba(Cu1/3Nb2/3)O3、Ba(W0.5Cu0.5)O3One of or a variety of sintering aids combination, And it must wherein contain Li2CO3。
2. bismuth ferrite-barium phthalate base high-temp leadless according to claim 1 with low-dielectric loss and high-temperature stability The preparation method of piezoelectric ceramics, it is characterized in that: preparation method includes the following steps:
(1) ingredient is carried out according to the component ratio of formula shown in composition general formula；
(2) it is medium by mixed-powder ball milling 24 hours of step (1) using dehydrated alcohol, in drying in 100 DEG C/6 hours, is put into height Aluminium crucible and compacting covers, and places into Muffle furnace with the heating rate of 250 DEG C/h to 800 DEG C, keeps the temperature 4 hours and synthesizes, and drops Temperature is taken out after being cooled to 200 DEG C or less；
(3) powder by step (2) synthesis carries out secondary ball milling 24 hours by medium of dehydrated alcohol, takes out drying；
(4) solution that mass percent concentration is 5%PVA is added in the powder after drying to be granulated, in punching block under 100MPa Compression moulding, mold interior diameter are 1cm；
(5) molding plain piece is to slowly warm up to 600 DEG C in tube furnace with the heating rate of 30 DEG C/h, keeps the temperature dumping for 24 hours, then With the heating rate of 20 DEG C/min to 980-1000 DEG C, 120min is kept the temperature, furnace cooling is then powered off；
(6) sintered sample is processed into two sides is smooth, thin slice of thickness 1mm, drapes over one's shoulders silver electrode, after 600 DEG C/30min silver ink firing It is spare；
(7) piezoelectric ceramic piece of preparation is polarized in silicone oil, polarized electric field 6000V/mm, 150 DEG C of temperature, the time 30 minutes, Electric field is kept to be cooled to room temperature.
3. a kind of bismuth ferrite with low-dielectric loss and high-temperature stability-barium phthalate base high-temp leadless piezoelectric ceramics, feature It is, forms general formula are as follows: (Bi1-wMw)(Fe1-tMe”'t)O3-xBaTiO3+yBi(Me”2/3M'1/3)O3+zBi(Zn0.5Ti0.5) O3+uNdCoO3+mP+nMnCO3, wherein x, y, z, u, m, n, t, w indicate molar fraction, 0 < x≤0.4,0≤y≤0.1,0 < z < 0.05,0≤u≤0.1,0 < m≤0.1,0 < n≤0.1,0≤w≤0.1,0≤t≤0.1, M is one in La, Er, Sm, Gd in formula Kind or it is several, Me " ' is one or more of trivalent metallic element Sc, In, Co and Ga, Me " be divalent metal element Ni, Mg, One of Zn, Sr, Pd, one of M' Nb, Ta, Sb, wherein P is B2O3、Li2CO3、V2O5、CuO、CeO2、LiBiO3、Ba (Cu1/3Nb2/3)O3、Ba(W0.5Cu0.5)O3One of or a variety of sintering aids combination, and must wherein contain Li2CO3。
4. bismuth ferrite-barium phthalate base high-temp leadless according to claim 3 with low-dielectric loss and high-temperature stability The preparation method of piezoelectric ceramics, it is characterized in that: preparation method includes the following steps:
(1) ingredient is carried out according to the component ratio of formula shown in composition general formula；
(2) it is medium by mixed-powder ball milling 24 hours of step (1) using dehydrated alcohol, in drying in 100 DEG C/6 hours, is put into height Aluminium crucible and compacting covers, and places into Muffle furnace with the heating rate of 250 DEG C/h to 800 DEG C, keeps the temperature 4 hours and synthesizes, and drops Temperature is taken out after being cooled to 200 DEG C or less；
(3) powder by step (2) synthesis carries out secondary ball milling 24 hours by medium of dehydrated alcohol, takes out drying；
(4) solution that mass percent concentration is 5%PVA is added in the powder after drying to be granulated, in punching block under 100MPa Compression moulding, mold interior diameter are 1cm；
(5) molding plain piece is to slowly warm up to 600 DEG C in tube furnace with the heating rate of 30 DEG C/h, keeps the temperature dumping for 24 hours, then With the heating rate of 20 DEG C/min to 980-1000 DEG C, 120min is kept the temperature, furnace cooling is then powered off；
(6) sintered sample is processed into two sides is smooth, thin slice of thickness 1mm, drapes over one's shoulders silver electrode, after 600 DEG C/30min silver ink firing It is spare；
(7) piezoelectric ceramic piece of preparation is polarized in silicone oil, polarized electric field 6000V/mm, 150 DEG C of temperature, the time 30 minutes, Electric field is kept to be cooled to room temperature.
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CN114577374B (en) * 2022-02-28 2023-12-29 福建工程学院 PVDF-based piezoelectric sensor and preparation method thereof
CN114751735A (en) * 2022-03-03 2022-07-15 常州大学 Dielectric energy storage ceramic powder, preparation method and application thereof in ceramic membrane
CN115073160A (en) * 2022-07-30 2022-09-20 桂林电子科技大学 High-performance bismuth ferrite-barium titanate ceramic with micro-nano electric domain structure and high service temperature zone and hot-pressing sintering preparation method thereof
CN115073160B (en) * 2022-07-30 2023-09-19 桂林电子科技大学 Hot-pressed sintering preparation method of bismuth ferrite-barium titanate ceramic with micro-nano electric domain structure
CN115849895A (en) * 2022-12-23 2023-03-28 吉林大学 Tantalum-magnesium-lanthanum-modified bismuth ferrite-based dielectric energy storage material and preparation method thereof
CN115849895B (en) * 2022-12-23 2023-09-29 吉林大学 Tantalum-magnesium-lanthanum modified bismuth ferrite-based dielectric energy storage material and preparation method thereof
CN118084473A (en) * 2024-04-26 2024-05-28 同济大学 Different-valence ion doped high-voltage electrical property lead-free bismuth ferrite-based piezoelectric ceramic material and preparation method thereof

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